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Electron-Beam-Induced Modifications in High-Density Polyethylene

Article in Brazilian Journal of Physics · May 2011

DOI: 10.1007/s13538-011-0004-7

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Braz J Phys (2011) 41:7–14
DOI 10.1007/s13538-011-0004-7
CONDENSED MATTER
Electron-Beam-Induced Modifications in High-Density
Polyethylene
H. G. Harish Kumar · R. D. Mathad · S. Ganesh ·
K. S. S. Sarma · C. R. Haramaghatti
Received: 4 July 2010 / Published online: 15 April 2011
© Sociedade Brasileira de Física 2011
Abstract Post-irradiation studies have been carried out
to elucidate the effects of electron beam irradiation on
the structural, optical, dielectric, and thermal proper-
ties of high-density polyethylene (HDPE) films. The
experimental results showed that both the optical band
gap and activation energy of HDPE films decreases
with an increase in the doses of electron radiation. The
electrical measurements showed that dielectric con-
stant and the ac conductivity of HDPE increases with
an increase in the dose of electron radiation. The ther-
mal analysis carried out using DSC and TGA revealed
that the melting temperature, degree of crystallinity,
and thermal stability of the HDPE films increased, ob-
viously, due to the predominant cross-linking reaction
following high doses of electron irradiation.
H. G. Harish Kumar (B) · R. D. Mathad
Department of Physics, Gulbarga University,
Gulbarga 585106, Karnataka, India
e-mail: harikumar_hg@rediffmail.com
R. D. Mathad
e-mail: rdmathad@yahoo.co.in
S. Ganesh
Microtron Center, Mangalore University,
Mangalore 574 199, India
K. S. S. Sarma
Bhabha Atomic Research Center,
Mumbai 400 085, India
C. R. Haramaghatti
Department of Inorganic and Physical Chemistry,
Indian Institute Science, Bangalore 560012, India
Keywords High-density polyethylene ·
Electron beam irradiation · UV-vis spectroscopy ·
Dielectric constant · Optical band gap ·
Activation energy
1 Introduction
Polymers, due to their high strength to weight ratio,
easy processability and excellent physical properties,
have been used in many applications such as in packag-
ing, electric cable insulations, microelectronics, dosime-
ter, and medical applications [1–3]. Furthermore, in
recent years there has been extensive utilization of
polymers in safety systems of nuclear power plants,
insulation of superconducting magnets used in fusion
reactors and in space applications [4]. In these appli-
cations polymers are often exposed to various kinds
of ionizing radiation, which results in the modifica-
tions in their physical properties. Therefore the studies
on ionizing radiation induced modifications in polymer
properties is gaining interest in recent years. Many
experimental investigations revealed that the interac-
tion of ionizing radiations with polymers lead to the
excitation and ionization of the atoms and molecules,
which cause subsequent rupture of the chemical bonds
resulting in the formation of polymer chain fragments
and free radicals. These transformations are responsi-
ble for most of the physical and/or chemical changes
observed in the polymers [5–18].
Among the thermoplastic polymers, the hydro-
genated polymers, such as polyethylene are of partic-
ular interests that are being employed in many com-
mercial and scientific applications. Polyethylene when
irradiated with the electron beam, gamma-rays, and
8 Braz J Phys (2011) 41:7–14
other forms of ionizing radiation predominately under-
goes cross-linking [19]. Furthermore, it is observed that
the irradiation of polyethylene leads to the creation
of polar groups on the polymer surface. Therefore, it
is important to study the effect of these dipoles on
the intensity of the optical transitions and dielectric
properties of polymers.
In the present work, we made an effort to study
the post irradiation effects on the structural, optical,
dielectric, and thermal properties of electron-irradiated
high-density polyethylene (HDPE) films over a dose
range of 0–360 kGy. The modifications in the optical
parameters viz., the optical band gap, activation en-
ergy, transition dipole moment, and oscillator strength
were investigated from the UV-Vis absorption spectral
analysis. Furthermore, the changes in the dielectric
and thermal properties of HDPE films irradiated at
different doses of electron radiation were respectively
studied using impedance analyzer, differential scanning
calorimeter (DSC) and thermo-gravimetric analyzer
(TGA).
2 Experimental
The HDPE samples in the form of granules was com-
pression molded into films of thicknesses 50 and 120 μm
using polymer press equipment (Technosearch, India,
PF-15). The compression molding was carried out by
placing the polymer granules between the stainless steel
dies at a temperature of 150◦ C under a pressure of
10 MPa for 10 min and was then cooled under pressure
by circulating water through the mold platens. The
samples were taken out when the platen temperature
reached 40◦ C. The films were stored in polyethylene
zipper packet and subjected to electron irradiation
using electron accelerator (ILU-6) at the Board of
Research in Isotope Technology (BRIT), Bhabha
Atomic Research Centre, Mumbai, India. The electron
beam of energy 1.2 MeV from the linear accelerator
was employed at 1.0 mA beam current to give a dose
rate of 10 kGy s−1 , and the films were irradiated sepa-
rately over the doses of 90, 180, 270 and 360 kGy. The
temperature of the samples during the irradiation was
maintained constant at about 25◦ C by breezing air onto
the samples.
The FTIR spectra of the pristine as well as the irra-
diated HDPE films were recorded using an FTIR spec-
trometer (Perkin–Elmer) over the wavenumber range
of 4,000–400 cm−1 with a resolution of 4 cm−1 .
The polymer samples of a thickness of 50 μm were
cut into a 1.0 × 4.0 cm2 dimension and inserted into a
quartz cell for recording the optical absorption spec-
tra using a UV–Vis spectrophotometer (Perkin–Elmer,
Lamda- 35). The absorption spectra were recorded
using an identical empty quartz cell as a reference over
the wavelength range of 190–500 nm.
The HDPE films of thickness 120 μm were cut into
dimension 1.0 × 1.0 cm2 and a thin coating of air drying
type silver paste was provided on both sides of the
films to achieve good electrical contact for dielectric
measurements. As the silver particles of the paste have
diameter of typically 1 μm, they stick to the sample sur-
face only and hence do not influence the conductivity
by interacting with the polymer. The samples were held
between two nominally spring loaded copper plates
and were subjected to dielectric measurements using
the LCR Hitester (HIOKI-3532-50) over the frequency
range of 100 Hz–1 MHz at the ambient temperature of
28◦ C. The values of the dielectric constant (ε  ) and ac
conductivity (σ ac ) were estimated from the measured
values of the capacitance (Cp ) and loss tangent (tanδ) at
the different frequencies using the following relations
ε = C p /C0 ; σ ac = 2π f C p Dt/A(ohm−1 cm−1 ) (1)
where C0 is the geometrical capacitance of vacuum of
the same dimensions as that of the sample; D = tan δ,
where δ being the phase angle; t, the thickness and A is
the cross-sectional area of the HDPE films. The DSC
measurements of both the pristine and the irradiated
HDPE samples were made using a Mettler Toledo
thermal analysis system. The samples weighing about
6.0 mg were scanned in the temperature range of 50–
600◦ C under nitrogen atmosphere at a heating rate of
10◦ C min−1 . The degree of crystallinity was calculated
using the following relation:
Hm
Xc = × 100 (2)
Hm
0
where Xc is the degree of crystallinity, Hm is the
specific enthalpy of melting and Hm ◦
(= 288 J g−1 )
is the specific melting enthalpy for 100% crystalline
HDPE [20].
The weight loss (%) was recorded as a function of
temperature for the pristine and the electron-beam-
irradiated HDPE samples using thermo gravimetric
analyzer (Mettler TA). The samples were cut into
very small pieces, crimped in small aluminum pans
and weighed in a microbalance with a precision up to
10 ppm. The samples were scanned in the temperature
range of 50–600◦ C with a heating rate of 20◦ C min−1 .
The resulting weight loss was recorded as a function of
temperature in terms of TGA thermograms.
Braz J Phys (2011) 41:7–14
3 Results and Discussions
3.1 Structural Analysis
We have given in Fig. 1 the FTIR transmission spec-
tra of the pristine and the electron irradiated HDPE
films over the wave number range 4,000–400 cm−1 . The
FTIR spectrum of the pristine HDPE films showed the
appearance of the strong bands in the wave number
region 2,830–2,950 cm−1 due to the C−H stretching
vibration of −CH2 group; the bands near ∼724 cm−1
due to the rocking deformation of long chain −CH2
group; the bands around at ∼1,463 cm−1 due to the
bending of −CH2 group; and the bands at ∼1,375 cm−1
due to the symmetrical bending of −CH3 group. The
FTIR spectra of irradiated HDPE films showed that the
intensity of most of the bands slightly increased with
theincrease in dose of electron radiation. Furthermore,
the occurrence of weak and strong bands around 3,440
cm−1 and 1,715 cm−1 indicated respectively the forma-
tion of oxidation hydroxyl (OH) and carbonyl (C=O)
groups as the electron irradiation of the polymer was
carried out in air. The co-existence of C=O and OH
groups suggested that the oxygen during the irradiation
resulted in the formation of peroxide radicals on the
Fig. 1 FTIR spectra for the pristine as well as the irradiated
HDPE films at different doses of electron radiation: a Pristine,
b 90 kGy, c 180 kGy, d 270 kGy, and e 360 kGy
9
polymer back bone. The increase in the intensity of
the band at 965 cm−1 corresponding to =C−H indi-
cated the creation of trans-vinylene group in the ir-
radiated samples. Further occurrence of the band at
∼1,640 cm−1 in the irradiated samples is due to the for-
mation of C=C bonds. Thus the appearance of new ab-
sorption bands in the irradiated HDPE films indicates
certainly the radiation induced structural modifications
in the polymer due to the breaking of molecular chains
leading to the increment of trans-vinylene unsaturation,
formation of carbonyl groups, and conjugated double
bonds.
3.2 Changes in Optical Properties
The UV-Vis absorption spectrum for the pristine as
well as the electron-beam-irradiated HDPE films over
the wavelength range 190–500 nm are given in Fig. 2.
The pristine HDPE has an absorption peak at ∼195 nm.
It is noticed that the height of the absorption peak in-
creases gradually and shifts slightly towards the longer
wavelength region upon electron irradiation. Further-
more, in increasing the dose of electron radiation,
broadening of the absorption peak was noticed. The
shift in the absorption edge towards the longer wave-
length region and broadening of peak for irradiated
polymers is generally attributed to the formation of
radicals, unsaturated bonds and possible formation of
carbon clusters.
Fig. 2 UV–Vis absorption spectrum for the pristine as well as the
irradiated HDPE films at different doses of electron radiation
10 Braz J Phys (2011) 41:7–14

Table 1 The estimated values of the optical band gap energy

In the high absorption region the absorption (Eg ), activation energy (Eu ), oscillator strength (f ), transition
coefficient (α) as a function of photon energy (hν) can dipole moment (μ) and number of carbon atom per cluster
be expressed as [21] size (N) for the pristine as well as the electron-beam-irradiated
HDPE films at different radiation doses
αhν = B(hν − Eg )r (3) Dose (kGy) Eg (eV) Eu (eV) f μ (Debye) N
0 5.44 2.459 1.04 6.5 ∼39
where (hν) is the incident photon energy, Eg the optical 90 4.69 1.9053 1.10 6.9 ∼53
band gap energy, B is a constant and r is an exponent 180 4.63 1.872 1.18 7.1 ∼55
which can take values 1/2, 3/2, 2, and 3 depending on 270 4.42 1.849 1.65 8.5 ∼60
the nature of the electronic transition responsible for 360 4.36 1.831 1.85 9.1 ∼62
the optical absorption. The best fit value of r can be
determined from the slope of the linear part of (αhν)1/r
versus hν. We obtained a best straight line fit to our the Robertson equation underestimates the cluster size
spectral data for r = 1/2, which indicated that a direct and hence they assumed the structure of the clusters to
transition is allowed. We estimated the values of the be like that of Buckminsterfullerene, C60 , instead of C6 ,
band gap energy from the extrapolation of the linear and arrived at the following relation given by
fit of straight line part of the plot of (αhν)2 versus √
hν to the zero absorption as shown in Fig. 3 and the Eg ≈ 34.3/ N (5)
estimated values of the Eg are given in Table 1. We
where N is the number of carbon atoms per cluster.
observe that the optical band gap of pristine HDPE
We used this relation to obtain the number of carbon
film decreased from 5.44 to 4.36 eV with increase in
atoms per cluster in the irradiated HDPE films, given in
the electron radiation dose. The decrease in the opti-
Table 1. Furthermore, in Fig. 2 one can observe that the
cal band gap of HDPE films with increasing dose of
absorption spectra showed an extending tail for lower
electron radiation could be attributed to the formation
photon energies below the band edge which can be
of chromophore groups (C=O) and extended systems
described by Urbach’s formula given by [24]
of conjugated bonds, e.g., carbon clusters as shown in
FTIR analysis. The number of carbon hexagon rings α = A exp(hν/Eu ) (6)
(M) in the cluster can be estimated from the Robertson
relation given by [22] where Eu is the activation energy which is a measure
of energy width of the tail of localized states in the
Eg = 2 |β| M−0.5 (4) band gap. Figure 4 shows a plot of (ln α) versus hν at
different electron radiation doses for the HDPE films.
where 2β is the band structure energy of a pair of The activation energy Eu was estimated from the recip-
adjacent π sites and β = −2.9 eV for six-membered rocal of the slope of the linear portion of the behavior
carbon ring, C6 . But Fink et al. [23] have shown that

Fig. 3 Plot of (αhν)2 versus hν for the pristine as well as the Fig. 4 Plot of (ln α) versus hν for the pristine as well as the
irradiated HDPE films at different doses of electron radiation irradiated HDPE films at different doses of electron radiation
Braz J Phys (2011) 41:7–14 11

of (ln α) with hν. The estimated values Eu are given the

Table 1.
Furthermore, the oscillator strength (f ), which ex-
press relative strength of the electronic transition
within the molecular system and is related to the inte-
grated molar absorption coefficient (ε) by the following
relation [25]

−9
f = 4.315 × 10 εdν (7)

where the molar absorption coefficient (ε) is equivalent

to (α/C) and C represents the molar concentration of
the material. Furthermore, the oscillator strength (f ) is
related to the dipole strength (D) of the transition by
the following expression [26]
 
4π me ν
f = D (8)
3e2 
where e is the electron charge, me , the electron mass
and ν, the frequency of transition. From the dipole
strength, one may then calculate the magnitude of the
transition dipole moment from valence band to conduc-
tion band using the following expression [26]
μ = D1/2
We have estimated the values of the oscillator
strength (f ) and the transition dipole moment (μ) for
the pristine as well as the irradiated HDPE films using
(7) and (9), respectively, whose values are presented in
Table 1. The plot of both the oscillator strength and
Fig. 6 Variation of transition dipole moment (μ) for HDPE films
irradiated at different dose of electron radiation
(9) the transition dipole moment as a function of electron
radiation dose are given in Figs. 5 and 6. It was observed
that both the oscillator strength and the transition di-
pole moment of HDPE increases with increase in the
dose of electron radiation. The value of f , in fact, is
found to increase from ∼1.04 for the pristine to ∼1.85
for the irradiated films and μ, from ∼6.5 Debye for
the pristine to ∼9.1 Debye for the irradiated HDPE
films at 360 kGy of electron radiation. The increase
in the oscillator strength confirms an increase in the
intensity of optical transitions in HDPE films upon
electron irradiation. The increase in both f and μ with
increasing electron dose could be attributed either to
the creation of new molecular dipoles as a result of for-
mation of point defects in the band gap of the polymer
or reorientation of the existing dipoles [27].

3.3 Modifications in Dielectric Properties

The variation of the dielectric constant (ε ) with log

Fig. 5 Variation of oscillator strength (f) for HDPE films irradi-
ated at different dose of electron radiation
frequency (log f ) for the pristine and the electron-
beam- irradiated HDPE films is given in Fig. 7. It can
be observed that the ε measured at 1 kHz increases
from 2.16 for the pristine to 2.91 for the irradiated
HDPE films at 360 kGy. The increase in dielectric
constant of HDPE films with the increase in electron
radiation doses might be attributed to scissoring of the
polymer molecular chains, which leads to the formation
of defect sites in the band gap of the polymer. These
defects could result in traps of charge carriers that
12
Fig. 7 Plot of dielectric constant (ε ) versus log f for HDPE films
irradiated at different doses of electron radiation
increase the ability of the polymer to store charges and
hence cause an increase in the dielectric constant of the
samples. The experimental results further showed that
the dielectric constant for the pristine as well as the
electron-beam-irradiated HDPE films decreases with
the increase in frequency. It might be observed that
as the frequency increases, the charge carriers migrate
through the dielectric and get trapped against a defect
site and induce an opposite charge in its vicinity and
thus the polarization of the trapped and the bound
charges cannot take place resulting in a decrease in the
dielectric constant at these frequencies.
Figure 8 depicts the dependence of the ac conduc-
tivity (σ ac ) on log frequency (log f ) at the ambient
Fig. 8 Plot of ac conductivity (σ ac ) versus log f for HDPE films
irradiated at different doses of electron radiation
Braz J Phys (2011) 41:7–14
temperature for both the pristine and the electron-
beam-irradiated HDPE samples. It is observed that σ ac
of the HDPE films increases slightly with increase in
the electron radiation dose and, in fact, a sharp increase
in the conductivity is observed above 105 Hz for all the
irradiated films. The increase in conductivity could be
due to the scissoring of polymer chains upon irradiation
which results in the formation of free radicals, unsatu-
rated bonds etc. This leads to an increase in the free-
charge carrier density in the polymer, which obviously
contributes to an enhancement in the ac conductivity of
the films at higher doses.
3.4 Modifications in Thermal Properties
The DSC thermograms for the pristine and the irradi-
ated HDPE samples at an electron radiation dose of
180 and 360 kGy are given in Fig. 9. The thermograms
showed changes in melting temperature and specific
enthalpy of melting of HDPE samples upon electron
irradiation. For the pristine samples the melting peak is
observed at 128.85◦ C and the degree of crystallinity es-
timated using (2) is about 63%. However upon electron
irradiation the melting temperature and specific heat
of enthalpy of HDPE found to increase with increase
in the dose of electron radiation. It is found that for
HDPE films irradiated at 360 kGy the melting temper-
ature increases to 133.42◦ C and degree of crystallinity
was also found to enhance to 67%. We have given
Fig. 9 DSC thermogram for the pristine and the irradiated
HDPE at 180 and 360 kGy dose of electron radiation
Braz J Phys (2011) 41:7–14
Table 2 DSC characterization of HDPE irradiated to different
dose of electron radiation
Dose Melting Heat of Degree of
(kGy) peak enthalpy crystallinity
(◦ C) (J g−1 ) (%)
0 128.85 183.83 ∼63
180 130.37 187.57 ∼65
360 133.43 192.56 ∼67
in Table 2 the melting temperatures as well as the
degree of crystallinity of HDPE samples irradiated at
different doses of electron radiation. The increase in
melting temperature in irradiated HDPE samples thus
indicates a predominant cross-linking of polymer chain
upon electron irradiation.
Furthermore, the increase in thermal stability in ir-
radiated HDPE samples was confirmed by TGA. We
have given the TGA thermograms for both the pristine
and the electron-irradiated HDPE samples at 180 and
360 kGy in Fig. 10. It is seen that for the pristine sample,
a slow decomposition zone is observed up to 300◦ C
where there is a weight loss of about 4%. A faster rate
of decomposition starts from 300◦ C till the polymer
is completely decomposed at 416◦ C where there is a
weight loss of about 86%. Similarly for the electron
irradiated HDPE at 360 kGy, a slower rate of decom-
position is noticed up to 415◦ C where the sample loses
about 11% of its initial weight. This is followed by a fast
decomposition over the range 415–484◦ C at which the
weight loss is about 89%. Thus, it is observed that the
thermal stability of HDPE increases due to the electron
beam irradiation. The reason for the increase in the
Fig. 10 TGA thermogram for the pristine and the irradiated
HDPE at dose of 180 and 360 kGy electron radiation
13
thermal behavior of the irradiated HDPE might be due
to the predominant cross-linking upon electron-beam-
irradiation which increases the molecular weight and
compactness of the polymer, imparting more strength
to withstand the thermal strain.
4 Conclusions
We conclude from the present studies that the electron-
beam irradiation modified the structural, optical, di-
electric and thermal properties of HDPE films. The
FTIR spectra showed the creation of trans-vinylene
unsaturation, carbonyl group and conjugated double
bonds in the electron-beam-irradiated of HDPE films.
The UV-Vis spectroscopic studies showed a decrease in
the optical band gap and activation energy of HDPE
films with increase in the dose of electron radiation.
Furthermore, an increase in the transition dipole mo-
ment and oscillator strength was observed in the irradi-
ated HDPE films due to the creation of new molecular
dipoles. The dielectric measurements further revealed
that the electron-beam irradiation resulted in a slight
increase in the dielectric constant and ac conductivity
of HDPE films upon electron irradiation which could
be attributed to the enhanced free electron density in
the irradiated samples as a consequence of molecular
chain scission, formation of free radicals and unsatu-
rated bonds. Furthermore, the DSC analysis showed
the increase in specific enthalpy of melting and degree
of crystallinity in irradiated HDPE and TGA analysis
indicated the occurrence of predominant cross-linking
in HDPE upon electron irradiation which increased the
thermal stability of irradiated samples.
Acknowledgements The authors are thankful to the Board of
Research in Nuclear Sciences (BRNS), Department of Atomic
Energy, Mumbai, India for providing the financial support under
Grant No. 2004/17-BRNS/1938. Our thanks are also due to the
personnel of BRIT, Mumbai, India for their help during the elec-
tron irradiation and also for providing the experimental facilities.
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